Scientists create “impossible material”—dubbed Upsalite—by accident

Reaction left over the weekend produces a material sought since the 1800s.

Researchers in Uppsala, Sweden, accidentally left a reaction running over the weekend and ended up solving a century-old chemistry problem. Their work has led to the development of new material, dubbed Upsalite, with remarkable water-binding properties. Upsalite promises to find applications in everything from humidity control at home to chemical manufacturing in industry.

Maria Strømme and colleagues at Uppsala University, whose work appears in the journal PLoS one, have modified a procedure dating back to 1908 to make a powdered and dry form of magnesium carbonate (MgCO3). The reaction ingredients are all cheaply available: magnesium oxide (MgO) and carbon dioxide (CO2), dissolved in methanol, a common industrial solvent. The result is pure, dry MgCO3.

Dry in this case means very dry. In the chemical sense, it means void of almost any water molecules at all.

Crystalline forms of dry MgCO3, which lack the structure needed to absorb water, are readily synthesized at high temperatures (over 100°C). As early as 1820, people started to search for lower-temperature routes to make dry MgCO3, but none have successfully yielded pure product until now. This is why Upsalite has been described as an “impossible material.”

The key modification was to increase the pressure of CO2 to three times that of normal atmospheric pressure, rather than simply bubbling the gas through a mixture of MgO in methanol. When one mixture was accidentally allowed to react over a long weekend, researchers came back to find a gel. It turns out the gel was formed because methanol molecules had been trapped within the material. When heated to 70°C, which is above the boiling point of methanol, the gel “solidifies and collapses into a white and coarse powder.” Analysis confirmed that the product was just what chemists had been trying to make for more than 100 years—a dry, powdered form of MgCO3.

Upsalite has impressive properties as a desiccant, absorbing water better than the much more expensive materials that are currently used (called zeolites). Most of the absorbed water is retained when Upsalite is transferred from a humid to a very dry environment. The dry form can be regenerated by heating to 95 °C. By contrast, most zeolites need to be heated to over 150 °C in order to dry them. Not only is Upsalite easy to make and reuse, but it is also non toxic to humans, which makes it suitable for use in humidity control indoors.

The impressive drying property stems from the very large internal surface area of Upsalite. MgCO3 is a common mineral that occurs in a variety of forms, most of which have water bound to their surface and are crystalline. By contrast, Upsalite has no water integrated into its structure and is not crystalline. Instead, it is mesoporous—a structure with pores that are a million times smaller than the width of a human hair—which provides it with a much greater surface area.

The past 20 years have seen a surge of interest in mesoporous materials such as zeolites and carbon nanotubes due to their ability to selectively absorb small molecules, which may enable applications in drug delivery, pollution removal, and the development of new catalysts for chemical reactions. Recognizing these prospects, the researchers have founded a spin-out company called Disruptive Materials to commercialize and apply Upsalite.

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I wonder if someone could explain a little better exactly how these desiccants are used in the real world, other then in little "do-no-eat" packets tossed into packaging. Obviously this stuff is way stronger than silica gel, but I'm not quite sure how you'd utilize it in, for example "humidity control indoors".

One critical step in air conditioning is removing water vapor. As you reduce temperature the relative humidity climbs which cam be uncomfortable at one end and actually dangerous at the other (imagine condensation forming on your electronics).

There are lots of ways around this. One is to overcool the air. Instead of bringing it to 70 degrees F you might bring it down to 55. Some of the water will condense out. You then heat the 55 deg. air back up to 70 deg. and it drops from saturated air (100% R.H. at 55) to something lower R.H. OF course, this consumes energy to have to over-cool the air.

Another option is to blow the 70 deg saturated (or just high RH) air through a desiccant trap. You have to use a material that can be regenerated - in this case you heat it up to release the water vapor and re-use it. You can't use something consumable. Obviously it requires energy to regenerate the water out of this material so it's a balancing act.

In industrial systems compressed air systems have to have desiccant traps to remove the excess water. In a similar fashion if I compress air I compress the water vapor as well. Compressors handle the liquid water that rains out but the output air is always saturated. That's not good for the equipment you're going to operate off the compressed air. In that case you run the air through a desiccant as well.

I'm glad that worked out as well as it did. Usually when a lab reaction is left unattended for a weekend, Something Bad happens and we need to be saved by a superhero.

Unless no superheroes are available, in which case the lab experiment goes from "Bad" to "Unpredictable" .. which creates a new superhero (and a super-villain, at the same time in an unconnected event in a nearby city)

In Norse mythology, Thor (from Old Norse Þórr) is a hammer-wielding god associated with thunder, lightning, storms, oak trees, strength, the protection of mankind, and also hallowing, healing and fertility.

So someone should update the wiki to add "desiccant".

Don't forget cross-dressing.

@ann_stone: Obviously not Thor from the movies. That's a fictional character.

Is anyone else concerned about the number of recent stories where suppposedly scientific labs have "accidentally" left mixtures of reagents sitting around unmonitored over a weekend? I thought labs were supposed to have protocols or something for this kind of stuff.

My wife work in reasearch and it is common to have experiments that need days to finish and these are usually left by themselves in the proper equipment, so if there are any issues the experiment is contained and isolated.

In other words, your wife's work wasn't accidental or unmonitored. It was science.

I wonder if someone could explain a little better exactly how these desiccants are used in the real world, other then in little "do-no-eat" packets tossed into packaging. Obviously this stuff is way stronger than silica gel, but I'm not quite sure how you'd utilize it in, for example "humidity control indoors".

Well, typically when we HVAC engineers try to control humidity, we're using a standard refrigeration cycle, in that we cool down the air going over an evaporator coil. The cold air holds less water than it could when it was warm, so the water condenses out on the evaporator coil. There's a limit to how much moisture you can effectively remove - but what if you could drive the air through an additional matrix of this desiccant material? Then you'd be be able to remove even more moisture. I don't know about the specific technologies and materials (I do HVAC design where I just pick out the specific units to install, I don't actually design the units). Anyway, the way this is typically done (from my imperfect understanding) is to have a desiccant wheel that's constantly rotating, where the airstream getting treated goes through one half of the wheel, and then a hot airstream goes through the other half of the wheel to "recharge" it. Question is, where does this heat come from? Well, you've got the heat that's being rejected by the AC system (through the condenser coil, which is outdoors on a typical "split system"), which is very convenient. So if you've got a rooftop unit (that is, all components are located in one unit on the exterior of the building) then you can have air being blown through the condenser coil to heat it up, and then further through the other half of the desiccant wheel, to drive the moisture from the wheel and "regenerate" it.

This article mentions specifically one advantage of this material being that it only has to be heated to 95C instead of over 150C, in order to dry it out, so it's might be a lot easier to integrate a desiccant wheel made of this stuff into a more mainstream piece of equipment.

Is anyone else concerned about the number of recent stories where suppposedly scientific labs have "accidentally" left mixtures of reagents sitting around unmonitored over a weekend? I thought labs were supposed to have protocols or something for this kind of stuff.

How many of our greatest inventions/discoveries in history were found by accident like this, before "lab protocols" and such were even in existence.

Not enough to outweigh the number of inventions/discoveries that couldn't be repeated, because nobody knew what really happened.

Is anyone else concerned about the number of recent stories where suppposedly scientific labs have "accidentally" left mixtures of reagents sitting around unmonitored over a weekend? I thought labs were supposed to have protocols or something for this kind of stuff.

How many of our greatest inventions/discoveries in history were found by accident like this, before "lab protocols" and such were even in existence.

Not enough to outweigh the number of inventions/discoveries that couldn't be repeated, because nobody knew what really happened.

If the conditions of the original accident can be repeated and provide the same results, it's still valid science because it results from designing an experiment (recreating the conditions) in order to test an hypothesis (that the accidental conditions bore the desirable yet unexpected results)

Depends on the jurisdiction and what they may try to claim in the patent application. I'm not sure if a USPTO Examiner would consider a different form of MgCO3 (i.e. dry powder versus dry crystal) to be a novel and non-obvious composition of matter. It might be. I can't even guess for the European Patent Office.

As for the process, I'm almost 100% sure that is patentable. Even if an examiner were to say, "increasing the pressure and increased duration of exposure is obvious", these scientists have a very solid rebuttal by saying, "well, if this process was so obvious, why didn't someone figure this out 100 years ago?"; the legal concept that applies is, "there was a long felt need in the field, which is a secondary indicia of nonobviousness".

I would have serious qualms with being able to patent the process. They were researchers at a public university, so they've already got a reward from the government, and we shouldn't give them another. Now, if they were to do further research based off of this and get patents on the results of that research, then it would be acceptable.

I would have serious qualms with being able to patent the process. They were researchers at a public university, so they've already got a reward from the government, and we shouldn't give them another. Now, if they were to do further research based off of this and get patents on the results of that research, then it would be acceptable.

This may be the single worst post I have ever read here. Ever.

You haven't been here long, then, have you? There have been far, FAR worse posts.

knbgnu does represent part of a valid and ongoing argument, though, whether government funded research should be allowed to be patented in the same way as privately funded research. If the public invests in research (albeit very indirect funding), shouldn't the public get the benefit without having to pay monopoly prices?

But wait! This was done accidently? Didn't anyone tell them that the United States Congress has determined that accidental discoveries that have useful business applications do not exist? They MUST go back in time and make sure Congress knows that they were fully planning on doing this.

Uppsala, Sweden. Not sure if the United States Congress has much sway over research in another country .

Magnesium sulfate = Epsom salts = laxative - A few spoonfuls in a glass of water is good exercise.Magnesium oxide. Don't wanna know about a few 100 grams, but it is sold as a dietary supplementin half or so gram pills.

Uppsala, Sweden. Not sure if the United States Congress has much sway over research in another country .

Julian Assange certainly seems to think that the US can fabricate rape accusations/convictions in Sweden and make Sweden deport him without a whole lot of due process. Otherwise, why would he be holed up in an embassy in London?

I think that the first non accidental experiment I would try would be to do supercritical solvent extraction to remove the methanol from the gel to (hopefully) create a magnesium carbonate aerogel.

The capillary pressure in small pores is enormous, so aerogels are made hydrophobic not to break apart due to stresses induced by moisture. They shed shards over time if left in normal climate untreated. Really difficult to get out of your fingers. With a really hydrophilic material it is probably worse.

In Norse mythology, Thor (from Old Norse Þórr) is a hammer-wielding god associated with thunder, lightning, storms, oak trees, strength, the protection of mankind, and also hallowing, healing and fertility.

So someone should update the wiki to add "desiccant".

Funny that it includes fertility, as one of the stories have Thor ask Odin why the latter gets all the ladies.

Is anyone else concerned about the number of recent stories where suppposedly scientific labs have "accidentally" left mixtures of reagents sitting around unmonitored over a weekend? I thought labs were supposed to have protocols or something for this kind of stuff.

Well, in this case, you could literally eat all the ingredients with little to no harm done (obviously, in moderate amounts), and the temperatures involved weren't very high (so little risk of a fire). If this involved hydrochloric acid at 200C, then yes, you'd want to put that away before leaving, but with these ingredients leaving them sit at worst might make cleanup slightly harder.

I wouldn't be quite as philosphical about eating (or drinking as the case may be) methanol But yeah - leaving a reaction running overnight or over a couple of days isn't a big deal. I suspect the 'accident' part of this was more 'hmmm that reaction didn't work the way we expected', rather than 'umm oops - who left that one running over the weekend?' In organic chemistry, the technical term for this kind of thing is 'brown smeg' because that's usually all you end up with rather than a massively useful side product